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The title complex, [Pd{(py)3COH}2](NO3)2, where (py)3COH is tris­(pyridin-2-yl)­methanol (C16H13N3O), studied at 150 and 298 K, has the potentially tridentate ligands present as bidentate ligands, with the Pd atom at a centre of symmetry. At 150 K, the Pd-N distances are 2.022 (3) and 2.026 (3) Å. The mean planes of the coordinated pyridine groups form dihedral angles of 42.1 (1) and 45.3 (1)° (at 150 K) with the coordination plane; the uncoordinated rings situated either side of the coordination plane form dihedral angles of 42.2 (1)° with it. The nitrate ions are regular and interact weakly with the hydroxyl group.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104010893/ta1448sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104010893/ta1448Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104010893/ta1448IIsup3.hkl
Contains datablock II

CCDC references: 245845; 245846

Comment top

Potentially tridentate `tripodal' ligands, such as (py)3CH (py is pyridin-2-yl), (pz)3CH (pz is pyrazol-1-yl) and [(pz)3BH], when coordinated to palladium(II) in the complexes [Pd{(py)3CH—N,N'}2](NO3)2, [Pd{(pz)3CH—N,N'}2](BF4)2 (both isomorphous) and [Pd{(pz)3BH—N,N'}2], may interact as bidentate ligands to give square-planar coordination for the metal atom (Canty et al., 1986). We have isolated a similar complex, the title compound, (I), with stoichiometry [Pd{(py)3COH}2(NO3)2], incorporating a ligand with added potential for interaction, and have examined its structure in a search for possible additional interaction at the Pd atom and elsewhere. We report here the X-ray analysis results for (I) at 150 and 298 K. \sch

Complex (I) crystallizes in space group P21/c, with similar cell dimensions to the earlier complexes. This is surprising, in view of the substitution of the methanic H atom by the polar hydroxyl group. The present complex thus provides a third member of this series of isomorphous complexes, in which the metal atom lies on a crystallographic inversion centre, with one half of the formula unit (half of the complex cation and a single nitrate ion) comprising the asymmetric unit of the structure (Figs. 1 and 2). The hydroxylic H atom and atom N2C aside, the cation symmetry is a good approximation to 2/m, Pd—N being effectively equivalent [2.022 (3) and 2.026 (3) Å at 150 K], with the chelate angle within the six-membered `boat' (atoms Pd and C1O Altered from C0 - Please check at the prows) being 87.2 (1)°. The torsion angles are given in Table 1. Geometries are generally harmonious with those found in the pair of isomorphous counterparts, with the uncoordinated ring shielding the Pd atom from the approach of other moieties. The hydroxyl group at the cation periphery interacts with the nitrate anion (Table 2), perhaps surprisingly since the uncoordinated pyridine offers, presumably, a more basic site.

As noted below, the present study was preceded by a room-temperature study on the same specimen. It is of interest to note, in comparing the two determinations, that, for all cation non-H atoms, all Ueq2) are less than 0.054 (3) at 298 K and less than 0.033 (3) at 150 K. For the nitrate ion, however, the Ueq values at 298 K are all greater than 0.101 (3), decreasing much more dramatically to be less than 0.049 (2) at 150 K. It is interesting to find that, at 150 K, the longest N—O distance in the anion, N—O2, is 1.261 (5) Å, perhaps consequent on the interaction with the hydroxyl H atom. The interplanar dihedral angles at 150 K (298 K) are rings A/B 56.9 (1) [58.1 (2)], A/C 75.0 (1) [76.8 (3)] and B/C 81.7 (1) [83.2 (2)]°. The deviations of the Pd atom from the planes of rings A and B are 0.097 (5) and 0.039 (5) Å [0.092 (10) and 0.012 (9) Å]. Rings A, B and C form dihedral angles of 42.1 (1) [43.0 (2)], 45.3 (1) [44.9 (2)] and 42.2 (1) [44.1 (2)°] with the coordination plane.

Experimental top

The white powder obtained from the reaction of PdMe2{(py)2COH} with water in acetone in the presence of pyridazine (Canty et al., 1994) was dissolved in methanol-water (Ratio?) and a few drops of dilute nitric acid. Colourless crystals of (I) formed over several days, and these were found to be suitable for structural studies. An initial determination, executed with a single counter instrument at room temperature on a capillary-mounted specimen, did not convincingly locate all H atoms. A fragment of the same specimen was used for a second determination using a CCD instrument, as reported here.

Refinement top

The H atoms were located in difference Fourier maps and placed at idealized positions (C—H = 0.95 Å), with Uiso(H) = 1.25Ueq(C). The largest peaks in the difference maps were 0.87 Å from Pd (at 150 K) and at the site of the Pd (at 298 K).

Computing details top

Data collection: SMART (Siemens, 1995) for (I); CAD-4 Software (Enraf-Nonius, 1989) for (II). Cell refinement: SAINT (Siemens, 1995) for (I); CAD-4 Software for (II). Data reduction: SAINT for (I); CAD-4 Software for (II). For both compounds, program(s) used to solve structure: Xtal3.5 (Hall et al., 1995); program(s) used to refine structure: CRYLSQ in Xtal3.5; molecular graphics: Xtal3.5; software used to prepare material for publication: BONDLA and CIFIO in Xtal3.5.

Figures top
[Figure 1] Fig. 1. The molecule of (I) at 150 K, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown with an arbitrary radii of 0.1 Å.
[Figure 2] Fig. 2. The unit-cell contents of (I) at 150 K, projected down b.
(I) Bis[tris(pyridin-2-yl)methanol-κ2N]palladium(II) dinitrate top
Crystal data top
[Pd(C16H13N3O)2](NO3)2F(000) = 768
Mr = 757.03Dx = 1.652 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -p 2ybcCell parameters from 4042 reflections
a = 8.428 (1) Åθ = 2.6–27.5°
b = 10.284 (2) ŵ = 0.68 mm1
c = 17.669 (3) ÅT = 150 K
β = 96.294 (2)°Block, colourless
V = 1522.2 (4) Å30.2 × 0.2 × 0.15 mm
Z = 2
Data collection top
Siemens SMART CCD area-detector
diffractometer
3681 independent reflections
Radiation source: sealed tube2726 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
ω scansθmax = 28.1°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.73, Tmax = 0.93k = 1313
17629 measured reflectionsl = 2323
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: difference Fourier map
wR(F2) = 0.117H-atom parameters constrained
S = 1.36 w = 1/[σ2(F) + 0.54F2]
2726 reflections(Δ/σ)max = 0.001
223 parametersΔρmax = 2.45 e Å3
0 restraintsΔρmin = 0.88 e Å3
0 constraints
Crystal data top
[Pd(C16H13N3O)2](NO3)2V = 1522.2 (4) Å3
Mr = 757.03Z = 2
Monoclinic, P21/cMo Kα radiation
a = 8.428 (1) ŵ = 0.68 mm1
b = 10.284 (2) ÅT = 150 K
c = 17.669 (3) Å0.2 × 0.2 × 0.15 mm
β = 96.294 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
3681 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2726 reflections with I > 2σ(I)
Tmin = 0.73, Tmax = 0.93Rint = 0.045
17629 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0480 restraints
wR(F2) = 0.117H-atom parameters constrained
S = 1.36Δρmax = 2.45 e Å3
2726 reflectionsΔρmin = 0.88 e Å3
223 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd0.500000.500000.500000.02062 (19)
C100.2922 (4)0.7445 (4)0.5132 (2)0.0236 (17)
O100.1936 (3)0.8537 (3)0.51290 (16)0.0289 (13)
C1A0.2181 (4)0.6272 (4)0.5498 (2)0.0237 (17)
N2A0.2940 (4)0.5111 (3)0.54846 (17)0.0215 (13)
C3A0.2358 (5)0.4079 (4)0.5831 (2)0.0272 (18)
C4A0.1006 (5)0.4161 (4)0.6210 (2)0.030 (2)
C5A0.0203 (5)0.5332 (5)0.6212 (2)0.034 (2)
C6A0.0781 (5)0.6395 (4)0.5844 (2)0.0290 (19)
C1B0.3070 (4)0.7141 (4)0.4291 (2)0.0231 (16)
N2B0.3917 (4)0.6085 (3)0.41359 (18)0.0234 (14)
C3B0.4059 (5)0.5756 (4)0.3408 (2)0.0260 (18)
C4B0.3359 (5)0.6485 (4)0.2806 (2)0.0277 (18)
C5B0.2501 (5)0.7577 (4)0.2960 (2)0.0306 (19)
C6B0.2342 (5)0.7922 (4)0.3705 (2)0.0283 (19)
C1C0.4585 (4)0.7735 (4)0.5558 (2)0.0236 (17)
N2C0.4794 (4)0.7364 (3)0.62928 (18)0.0275 (16)
C3C0.6191 (5)0.7661 (4)0.6700 (2)0.030 (2)
C4C0.7412 (5)0.8314 (4)0.6391 (2)0.032 (2)
C5C0.7169 (5)0.8709 (4)0.5643 (2)0.0302 (19)
C6C0.5726 (5)0.8427 (4)0.5215 (2)0.0281 (18)
N0.1648 (4)1.0631 (3)0.6658 (2)0.0292 (17)
O10.2944 (4)1.0990 (4)0.6443 (2)0.049 (2)
O20.1009 (4)0.9601 (3)0.6384 (2)0.0418 (17)
O30.1023 (4)1.1251 (3)0.71392 (18)0.0408 (17)
H100.181970.884080.558840.04400*
H3C0.634320.729640.721120.02300*
H3A0.287940.327140.581590.04300*
H4A0.063600.342720.646330.02500*
H5A0.073660.540880.645950.02600*
H6A0.023370.719810.583010.03200*
H3B0.465510.500920.330580.02700*
H4B0.346440.623980.229800.01200*
H5B0.202270.809370.255190.04300*
H6B0.175030.866790.381450.02000*
H4C0.839140.847680.668370.03200*
H5C0.798400.917490.542770.05400*
H6C0.552280.869430.469960.03000*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd0.0230 (2)0.0190 (2)0.0196 (2)0.00086 (17)0.00143 (13)0.00056 (16)
C100.0228 (17)0.0243 (18)0.0231 (17)0.0045 (14)0.0002 (13)0.0008 (14)
O100.0318 (15)0.0272 (14)0.0273 (14)0.0094 (12)0.0010 (11)0.0012 (11)
C1A0.0245 (17)0.0253 (18)0.0206 (17)0.0010 (15)0.0013 (13)0.0033 (14)
N2A0.0245 (14)0.0208 (15)0.0191 (13)0.0016 (13)0.0019 (11)0.0012 (12)
C3A0.0271 (19)0.0233 (18)0.031 (2)0.0029 (15)0.0017 (15)0.0026 (15)
C4A0.034 (2)0.032 (2)0.0246 (19)0.0081 (17)0.0030 (16)0.0032 (16)
C5A0.027 (2)0.045 (3)0.030 (2)0.0043 (17)0.0055 (16)0.0060 (17)
C6A0.028 (2)0.031 (2)0.027 (2)0.0025 (16)0.0006 (15)0.0038 (16)
C1B0.0245 (18)0.0204 (17)0.0240 (17)0.0013 (14)0.0005 (14)0.0017 (14)
N2B0.0237 (15)0.0227 (16)0.0231 (15)0.0011 (12)0.0004 (12)0.0012 (12)
C3B0.030 (2)0.0256 (19)0.0220 (17)0.0027 (15)0.0023 (14)0.0020 (14)
C4B0.029 (2)0.032 (2)0.0211 (17)0.0068 (16)0.0001 (14)0.0010 (15)
C5B0.032 (2)0.032 (2)0.0260 (19)0.0046 (17)0.0052 (15)0.0062 (16)
C6B0.0258 (19)0.030 (2)0.028 (2)0.0027 (16)0.0021 (15)0.0000 (16)
C1C0.0253 (18)0.0212 (18)0.0236 (17)0.0033 (14)0.0006 (14)0.0021 (14)
N2C0.0290 (17)0.0289 (17)0.0239 (16)0.0006 (14)0.0002 (13)0.0001 (13)
C3C0.031 (2)0.032 (2)0.026 (2)0.0012 (17)0.0010 (16)0.0012 (16)
C4C0.027 (2)0.033 (2)0.035 (2)0.0017 (17)0.0056 (16)0.0020 (18)
C5C0.031 (2)0.0221 (18)0.037 (2)0.0037 (16)0.0036 (16)0.0015 (16)
C6C0.036 (2)0.0228 (18)0.0252 (18)0.0001 (16)0.0017 (16)0.0037 (15)
N0.0322 (17)0.0250 (18)0.0306 (18)0.0056 (14)0.0041 (14)0.0051 (14)
O10.049 (2)0.045 (2)0.057 (2)0.0066 (16)0.0178 (17)0.0039 (17)
O20.0446 (19)0.0373 (17)0.0427 (19)0.0046 (15)0.0013 (15)0.0119 (14)
O30.0442 (18)0.0429 (19)0.0345 (16)0.0104 (15)0.0006 (14)0.0086 (14)
Geometric parameters (Å, º) top
Pd—N2A2.022 (3)N2B—C3B1.347 (5)
Pd—N2B2.026 (3)C3B—C4B1.381 (5)
Pd—N2A2.022 (3)C3B—H3B0.946
Pd—N2B2.026 (3)C4B—C5B1.378 (6)
C10—O101.396 (5)C4B—H4B0.946
C10—C1A1.534 (6)C5B—C6B1.384 (6)
C10—C1B1.538 (5)C5B—H5B0.949
C10—C1C1.545 (5)C6B—H6B0.947
O10—H100.885C1C—N2C1.345 (5)
C1A—N2A1.355 (5)C1C—C6C1.389 (6)
C1A—C6A1.394 (6)N2C—C3C1.346 (5)
N2A—C3A1.345 (5)C3C—C4C1.390 (6)
C3A—C4A1.386 (6)C3C—H3C0.973
C3A—H3A0.941C4C—C5C1.377 (6)
C4A—C5A1.382 (6)C4C—H4C0.939
C4A—H4A0.947C5C—C6C1.391 (6)
C5A—C6A1.387 (6)C5C—H5C0.950
C5A—H5A0.949C6C—H6C0.948
C6A—H6A0.945N—O11.250 (5)
C1B—N2B1.345 (5)N—O21.261 (5)
C1B—C6B1.397 (5)N—O31.227 (5)
N2A—Pd—N2B87.20 (12)Pd—N2B—C1B119.8 (3)
N2A—Pd—N2A180.0000Pd—N2B—C3B120.1 (3)
N2A—Pd—N2B92.80 (12)C1B—N2B—C3B120.1 (3)
N2B—Pd—N2A92.80 (12)N2B—C3B—C4B121.6 (4)
N2B—Pd—N2B180.0000N2B—C3B—H3B119.4
N2A—Pd—N2B87.20 (12)C4B—C3B—H3B119.0
O10—C10—C1A111.4 (3)C3B—C4B—C5B118.7 (4)
O10—C10—C1B105.7 (3)C3B—C4B—H4B120.6
O10—C10—C1C110.8 (3)C5B—C4B—H4B120.7
C1A—C10—C1B109.1 (3)C4B—C5B—C6B120.2 (4)
C1A—C10—C1C109.6 (3)C4B—C5B—H5B119.6
C1B—C10—C1C110.2 (3)C6B—C5B—H5B120.1
C10—O10—H10113.9C1B—C6B—C5B118.5 (4)
C10—C1A—N2A118.1 (3)C1B—C6B—H6B120.8
C10—C1A—C6A121.1 (4)C5B—C6B—H6B120.7
N2A—C1A—C6A120.8 (4)C10—C1C—N2C115.5 (3)
Pd—N2A—C1A119.1 (3)C10—C1C—C6C121.3 (3)
Pd—N2A—C3A121.4 (3)N2C—C1C—C6C122.9 (3)
C1A—N2A—C3A119.4 (3)C1C—N2C—C3C117.8 (4)
N2A—C3A—C4A122.1 (4)N2C—C3C—C4C122.8 (4)
N2A—C3A—H3A119.3N2C—C3C—H3C115.3
C4A—C3A—H3A118.6C4C—C3C—H3C121.5
C3A—C4A—C5A118.9 (4)C3C—C4C—C5C118.8 (4)
C3A—C4A—H4A120.7C3C—C4C—H4C120.9
C5A—C4A—H4A120.4C5C—C4C—H4C120.4
C4A—C5A—C6A119.3 (4)C4C—C5C—C6C119.4 (4)
C4A—C5A—H5A120.5C4C—C5C—H5C119.7
C6A—C5A—H5A120.3C6C—C5C—H5C121.0
C1A—C6A—C5A119.4 (4)C1C—C6C—C5C118.4 (4)
C1A—C6A—H6A120.2C1C—C6C—H6C120.5
C5A—C6A—H6A120.4C5C—C6C—H6C121.1
C10—C1B—N2B117.5 (3)O1—N—O2118.8 (4)
C10—C1B—C6B121.6 (3)O1—N—O3120.9 (4)
N2B—C1B—C6B120.9 (4)O2—N—O3120.3 (4)
N2B—Pd—N2A—C1A44.5 (3)C1A—C10—C1B—N2B57.4 (4)
N2A—Pd—N2B—C1B45.5 (3)C10—C1A—N2A—Pd0.7 (4)
C1B—C10—C1A—N2A58.3 (4)C10—C1B—N2B—Pd2.0 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10···O20.891.812.666 (5)163
(II) Bis[tris(pyridin-2-yl)methanol-κ2N]palladium(II) dinitrate top
Crystal data top
[Pd(C16H13N3O)2](NO3)2F(000) = 768
Mr = 757.03Dx = 1.626 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -p 2ybcCell parameters from 6 reflections
a = 8.430 (3) Åθ = 12.2–16.3°
b = 10.431 (4) ŵ = 0.67 mm1
c = 17.67 (2) ÅT = 298 K
β = 95.54 (6)°Block, colourless
V = 1546.5 (19) Å30.25 × 0.22 × 0.19 mm
Z = 2
Data collection top
Enraf-Nonius CAD-4
diffractometer
2323 reflections with I > 2σ(I)
Radiation source: rotating anodeRint = 0.086
Graphite monochromatorθmax = 30.0°, θmin = 2.3°
2θω scansh = 010
Absorption correction: gaussian
ABSORB in Xtal3.5 (Hall et al., 1995)
k = 014
Tmin = 0.85, Tmax = 0.88l = 2424
4422 measured reflections8 standard reflections every 60 min
4414 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.056Hydrogen site location: difference Fourier map
wR(F2) = 0.145H-atom parameters constrained
S = 1.59 w = 1/[σ2(F) + 0.84F2]
2323 reflections(Δ/σ)max = 0.001
223 parametersΔρmax = 1.38 e Å3
0 restraintsΔρmin = 0.79 e Å3
0 constraints
Crystal data top
[Pd(C16H13N3O)2](NO3)2V = 1546.5 (19) Å3
Mr = 757.03Z = 2
Monoclinic, P21/cMo Kα radiation
a = 8.430 (3) ŵ = 0.67 mm1
b = 10.431 (4) ÅT = 298 K
c = 17.67 (2) Å0.25 × 0.22 × 0.19 mm
β = 95.54 (6)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
2323 reflections with I > 2σ(I)
Absorption correction: gaussian
ABSORB in Xtal3.5 (Hall et al., 1995)
Rint = 0.086
Tmin = 0.85, Tmax = 0.888 standard reflections every 60 min
4422 measured reflections intensity decay: none
4414 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0560 restraints
wR(F2) = 0.145H-atom parameters constrained
S = 1.59Δρmax = 1.38 e Å3
2323 reflectionsΔρmin = 0.79 e Å3
223 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd0.500000.500000.500000.0303 (3)
C100.2979 (7)0.7427 (6)0.5144 (4)0.033 (3)
O100.1991 (6)0.8516 (5)0.5151 (3)0.049 (3)
C1A0.2212 (7)0.6292 (7)0.5514 (4)0.034 (3)
N2A0.2939 (6)0.5152 (6)0.5489 (3)0.033 (2)
C3A0.2320 (8)0.4123 (7)0.5828 (4)0.043 (4)
C4A0.0965 (10)0.4221 (9)0.6207 (5)0.054 (5)
C5A0.0213 (10)0.5376 (9)0.6217 (5)0.059 (5)
C6A0.0830 (9)0.6427 (8)0.5869 (4)0.048 (4)
C1B0.3122 (8)0.7132 (6)0.4310 (4)0.036 (3)
N2B0.3956 (6)0.6079 (5)0.4152 (3)0.036 (3)
C3B0.4078 (9)0.5762 (7)0.3418 (4)0.042 (3)
C4B0.3390 (9)0.6490 (8)0.2832 (4)0.048 (4)
C5B0.2542 (10)0.7569 (8)0.2994 (4)0.053 (4)
C6B0.2407 (9)0.7886 (8)0.3736 (5)0.048 (4)
C1C0.4620 (8)0.7718 (6)0.5565 (4)0.035 (3)
N2C0.4824 (7)0.7335 (6)0.6289 (3)0.045 (3)
C3C0.6206 (10)0.7644 (8)0.6689 (4)0.052 (4)
C4C0.7414 (10)0.8315 (9)0.6383 (5)0.054 (5)
C5C0.7188 (9)0.8705 (8)0.5639 (5)0.053 (4)
C6C0.5766 (9)0.8407 (7)0.5221 (4)0.043 (3)
N0.8347 (8)0.5602 (7)0.8367 (4)0.049 (3)
O10.7087 (12)0.5856 (13)0.8598 (6)0.134 (8)
O20.9012 (11)0.4627 (7)0.8588 (6)0.100 (6)
O30.8904 (10)0.6298 (9)0.7905 (4)0.096 (5)
H100.214100.877200.566600.08000*
H3A0.282570.329370.578460.05300*
H4A0.058200.348830.648280.06600*
H5A0.076820.544810.645160.07700*
H6A0.031560.726970.589260.06100*
H3B0.468280.501050.330410.05400*
H4B0.346930.623210.230790.06000*
H5B0.207410.808720.257000.06600*
H6B0.178430.863300.386200.05900*
H3C0.637520.737170.721820.06500*
H4C0.837540.851950.668950.06400*
H5C0.801560.917330.541270.06600*
H6C0.557880.867220.469810.05500*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd0.0312 (3)0.0316 (3)0.0288 (3)0.0024 (4)0.00716 (18)0.0011 (4)
C100.031 (3)0.030 (3)0.038 (3)0.004 (2)0.001 (2)0.001 (2)
O100.052 (3)0.045 (3)0.050 (3)0.022 (2)0.000 (2)0.001 (2)
C1A0.027 (3)0.044 (4)0.031 (3)0.004 (3)0.004 (2)0.002 (3)
N2A0.033 (2)0.031 (3)0.037 (2)0.002 (2)0.0066 (17)0.002 (2)
C3A0.039 (4)0.042 (4)0.049 (4)0.009 (3)0.007 (3)0.005 (3)
C4A0.045 (4)0.060 (5)0.057 (5)0.013 (4)0.010 (4)0.003 (4)
C5A0.039 (4)0.075 (6)0.063 (5)0.010 (4)0.015 (3)0.011 (4)
C6A0.038 (4)0.058 (5)0.049 (4)0.005 (3)0.009 (3)0.006 (4)
C1B0.034 (3)0.032 (3)0.041 (3)0.002 (2)0.003 (3)0.002 (3)
N2B0.037 (3)0.041 (3)0.031 (2)0.006 (2)0.005 (2)0.003 (2)
C3B0.049 (4)0.046 (4)0.033 (3)0.002 (3)0.007 (3)0.003 (3)
C4B0.050 (4)0.059 (5)0.036 (3)0.011 (4)0.006 (3)0.001 (3)
C5B0.058 (5)0.060 (5)0.040 (4)0.000 (4)0.001 (3)0.012 (3)
C6B0.045 (4)0.050 (5)0.049 (4)0.005 (3)0.002 (3)0.012 (4)
C1C0.039 (3)0.027 (3)0.039 (3)0.005 (2)0.004 (3)0.002 (2)
N2C0.045 (3)0.055 (4)0.034 (3)0.001 (3)0.002 (2)0.002 (3)
C3C0.050 (4)0.060 (5)0.045 (4)0.001 (4)0.001 (3)0.006 (4)
C4C0.047 (4)0.052 (5)0.061 (5)0.005 (4)0.003 (4)0.014 (4)
C5C0.045 (4)0.044 (4)0.072 (5)0.009 (3)0.012 (4)0.002 (4)
C6C0.048 (4)0.039 (4)0.042 (4)0.008 (3)0.007 (3)0.002 (3)
N0.054 (4)0.048 (4)0.046 (3)0.008 (3)0.006 (3)0.003 (3)
O10.101 (7)0.191 (11)0.118 (7)0.004 (7)0.056 (6)0.053 (8)
O20.110 (7)0.066 (5)0.118 (7)0.023 (4)0.018 (5)0.014 (4)
O30.108 (6)0.103 (6)0.075 (4)0.043 (5)0.002 (4)0.031 (4)
Geometric parameters (Å, º) top
Pd—N2A2.020 (5)N2B—C3B1.351 (9)
Pd—N2B2.008 (5)C3B—C4B1.367 (10)
Pd—N2A2.020 (5)C3B—H3B0.967
Pd—N2B2.008 (5)C4B—C5B1.379 (12)
C10—O101.409 (8)C4B—H4B0.972
C10—C1A1.527 (9)C5B—C6B1.367 (12)
C10—C1B1.521 (9)C5B—H5B0.976
C10—C1C1.536 (8)C6B—H6B0.977
O10—H100.944C1C—N2C1.335 (9)
C1A—N2A1.341 (9)C1C—C6C1.390 (10)
C1A—C6A1.382 (10)N2C—C3C1.342 (10)
N2A—C3A1.357 (10)C3C—C4C1.388 (12)
C3A—C4A1.382 (12)C3C—H3C0.974
C3A—H3A0.970C4C—C5C1.371 (13)
C4A—C5A1.362 (13)C4C—H4C0.955
C4A—H4A0.979C5C—C6C1.381 (11)
C5A—C6A1.382 (13)C5C—H5C0.969
C5A—H5A0.963C6C—H6C0.963
C6A—H6A0.983N—O11.204 (13)
C1B—N2B1.348 (9)N—O21.208 (11)
C1B—C6B1.375 (10)N—O31.220 (11)
N2A—Pd—N2B86.7 (2)Pd—N2B—C1B120.1 (4)
N2A—Pd—N2A180.0000Pd—N2B—C3B120.7 (5)
N2A—Pd—N2B93.3 (2)C1B—N2B—C3B119.2 (6)
N2B—Pd—N2A93.3 (2)N2B—C3B—C4B121.7 (7)
N2B—Pd—N2B180.0000N2B—C3B—H3B119.2
N2A—Pd—N2B86.7 (2)C4B—C3B—H3B119.1
O10—C10—C1A110.2 (5)C3B—C4B—C5B119.0 (7)
O10—C10—C1B106.0 (5)C3B—C4B—H4B120.3
O10—C10—C1C110.0 (5)C5B—C4B—H4B120.6
C1A—C10—C1B109.6 (5)C4B—C5B—C6B119.4 (7)
C1A—C10—C1C110.1 (5)C4B—C5B—H5B118.1
C1B—C10—C1C110.9 (5)C6B—C5B—H5B122.6
C10—O10—H10102.3C1B—C6B—C5B119.8 (8)
C10—C1A—N2A117.4 (5)C1B—C6B—H6B119.7
C10—C1A—C6A121.8 (6)C5B—C6B—H6B120.4
N2A—C1A—C6A120.9 (7)C10—C1C—N2C115.6 (6)
Pd—N2A—C1A119.9 (4)C10—C1C—C6C121.5 (6)
Pd—N2A—C3A120.6 (5)N2C—C1C—C6C122.8 (6)
C1A—N2A—C3A119.4 (6)C1C—N2C—C3C117.3 (6)
N2A—C3A—C4A121.7 (7)N2C—C3C—C4C123.2 (7)
N2A—C3A—H3A118.7N2C—C3C—H3C118.4
C4A—C3A—H3A119.6C4C—C3C—H3C118.4
C3A—C4A—C5A118.7 (8)C3C—C4C—C5C119.0 (8)
C3A—C4A—H4A120.7C3C—C4C—H4C120.4
C5A—C4A—H4A120.5C5C—C4C—H4C120.6
C4A—C5A—C6A120.0 (8)C4C—C5C—C6C118.6 (8)
C4A—C5A—H5A119.6C4C—C5C—H5C120.4
C6A—C5A—H5A120.3C6C—C5C—H5C121.0
C1A—C6A—C5A119.4 (8)C1C—C6C—C5C119.1 (7)
C1A—C6A—H6A120.3C1C—C6C—H6C120.7
C5A—C6A—H6A120.3C5C—C6C—H6C120.1
C10—C1B—N2B117.2 (5)O1—N—O2118.3 (9)
C10—C1B—C6B121.8 (6)O1—N—O3120.3 (9)
N2B—C1B—C6B120.9 (6)O2—N—O3121.4 (9)

Experimental details

(I)(II)
Crystal data
Chemical formula[Pd(C16H13N3O)2](NO3)2[Pd(C16H13N3O)2](NO3)2
Mr757.03757.03
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)150298
a, b, c (Å)8.428 (1), 10.284 (2), 17.669 (3)8.430 (3), 10.431 (4), 17.67 (2)
β (°) 96.294 (2) 95.54 (6)
V3)1522.2 (4)1546.5 (19)
Z22
Radiation typeMo KαMo Kα
µ (mm1)0.680.67
Crystal size (mm)0.2 × 0.2 × 0.150.25 × 0.22 × 0.19
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Enraf-Nonius CAD-4
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Gaussian
ABSORB in Xtal3.5 (Hall et al., 1995)
Tmin, Tmax0.73, 0.930.85, 0.88
No. of measured, independent and
observed [I > 2σ(I)] reflections
17629, 3681, 2726 4422, 4414, 2323
Rint0.0450.086
(sin θ/λ)max1)0.6620.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.048, 0.117, 1.36 0.056, 0.145, 1.59
No. of reflections27262323
No. of parameters223223
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.45, 0.881.38, 0.79

Computer programs: SMART (Siemens, 1995), CAD-4 Software (Enraf-Nonius, 1989), SAINT (Siemens, 1995), CAD-4 Software, SAINT, Xtal3.5 (Hall et al., 1995), CRYLSQ in Xtal3.5, BONDLA and CIFIO in Xtal3.5.

Selected geometric parameters (Å, º) for (I) top
Pd—N2A2.022 (3)Pd—N2B2.026 (3)
N2A—Pd—N2B87.20 (12)
N2B—Pd—N2A—C1A44.5 (3)C1A—C10—C1B—N2B57.4 (4)
N2A—Pd—N2B—C1B45.5 (3)C10—C1A—N2A—Pd0.7 (4)
C1B—C10—C1A—N2A58.3 (4)C10—C1B—N2B—Pd2.0 (4)
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O10—H10···O20.891.812.666 (5)163
 

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